Friday, February 20, 2009

Bio diesel analysis and European Standard EN14214

A Metrohm UK product story
Edited by the Laboratorytalk editorial team May 4, 2006

Manufacture and use of fatty acid methyl esters (Fame), has huge implications for the environment; biodiesel is a clean burning alternative fuel, produced from domestic, renewable resources

Bio diesel contains no petroleum, but it can be blended at any level with petroleum diesel to create a bio diesel blend.
It can be used in compression-ignition (diesel) engines with little or no modifications.
Bio diesel is simple to use, biodegradable, non-toxic, and essentially free of sulphur and aromatics.
Bio diesel is made through a chemical process called transesterification whereby the glycerine is separated from the fat or vegetable oil.
The process leaves behind two products - methyl esters (the chemical name for bio diesel) and glycerine (a valuable by-product usually sold to be used in soaps and other products).
Fuel-grade bio diesel must be produced to strict industry specifications (ASTM D6751) in order to insure proper performance.
Bio diesel is the only alternative fuel to have fully completed the health effects testing requirements of the 1990 Clean Air Act Amendments.
Bio diesel that meets ASTM D6751 and is legally registered with the Environmental Protection Agency is a legal motor fuel for sale and distribution.
Metrohm can offer a solution to many of the analytical requirements listed in European Standard EN14214, namely:.
Oxidative stability rancimat method.
Acid value potentiometric titration.
Iodine value potentiometric titration.
Water content Karl Fischer.
Viscosity rotational viscometers.
Oxidative Stability.
The Metrohm Rancimat 743 method for measuring the oxidative stability of fatty acid methyl esters is determined according to DIN EN 14112.
In this method the highly volatile organic acids produced by autoxidation are absorbed in water and used to indicate induction time.
With the simple to use 743 Rancimat, the determination takes place at a highly sophisticated level.
Eight measuring positions in two independent heating blocks.
Individual start on each position.
Comprehensive control by PC.
Up to four Rancimat measuring blocks per PC - and therefore up to 32 samples at up to eight different temperatures.
Integrated GLP Test.
Titrations for bio diesel.
As listed in European Standard EN14214, Bio diesel manufacturers are required to determine acid value and iodine number by titration.
Using Metrohm autotitrators these methods have been perfected over the years and can be found in Metrohm Application Bulletin 141- Analysis of Edible Oils and Fats.
Iodine number.
For this analysis the following are required.
Metrohm Autotitrator, either a Titrando or a Titrino Model.
Combined Platinum Electrode e.g Pt Titrode or Pt Ring Electrodes.
The titration is a dynamic (DET U) Back titration with 0.1M Sodium Thiosulphate.
The sample is dissolve sample in Glacial Acetic Acid.
And added are 25ml of reaction solution and 10ml catalyst.
(specified in Bulletin).
Store in dark for five minutes.
Add 15ml KI solution, DI water and back-titrate to excess of iodine with 0.1M Na2S2O3.
At same time run a blank without sample.
The titrator automatically carries out the calculation g iodine/100g =(ml of thiosulphate for blank - ml thiosulphate for sample) x 1.269/ sample size (1.269=equivalent weight of iodine).
Acid Number.
You will need.
Autotitrator- Titrando or Titrino Models.
Solvotrode Non-aqueous pH electrode with LiCl sat.
in ethanol electrolyte.
0.1M KOH in isopropanol.
Solvent mixture ethanol/diethyl ether 1:1.
Weigh out 5-10 g sample, dissolve in 50ml solvent mixture.
Dynamic (DET U) Titration with KOH.
AN mgKOH/g = ml 0.1M KOH x 5.61/ sample size (5.61=equivalent weight KOH).
Karl Fischer moisture analysis.
EN14214/ EN ISO 12937 states that water determination should be by coulometric KF titration method.
Metrohm can offer a choice of two Coulometers, either the 831 or the 756 models.
In some cases the addition of a solubility promoter (chloroform or propanol) is recommended to improve solubility.

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